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Volume 19, Issue 8
Displaying 1-22 of 22 articles from this issue
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Possibility of determination of carbon with carbon spectrum (above 2, 000 A) in ultraviolet and visual regionHidehiro GOTO, Kichinosuke HIROKAWA, Kunio TAKADA1970 Volume 19 Issue 8 Pages 1021-1026
Published: August 05, 1970
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSIt is possible to simultaneously determine carbon and other metals if carbon is determined with no vacuum spectrograph. Therefore, possibility of analysis of carbon in steel by low voltage impulse discharge was studied with carbon spectrum in ultraviolet and visual region. The best carbon line in 20007000Å was CIII 2296.89Å and it was not influence by closed iron spectra. FeII 2481.05Å, FeII 2481.57Å, FeII 2497.30Å and FeII 2568.40Å were selected as internal lines. The favorable excitation conditions were 400 V (D. C.), 2000 μF, 50 μH, sample negative and in helium atmosphere.
Under those conditions, carbon in steel of 0.01% to 1.0% was determined, and coefficient of variation of sample containing 0.084% carbon was about 16%.View full abstractDownload PDF (894K) -
Masayoshi EZAWA1970 Volume 19 Issue 8 Pages 1026-1031
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA spectrophotometric method has been proposed for the determination of chromium in yttrium vanadate phosphor, and the recommended procedure is as follows. Dissolve 0.1 to 0.15 g of sample in conc. sulfuric acid, evaporate to fumes, and dilute to 100 ml with deionized water. To the 20 ml of test solution and 3 ml of sulfuric acid and 2 ml of 30% aqueous hydrogen peroxide. Boil to decompose hydrogen peroxide for 5 min, and evaporate to 15 ml.
Transfer the solution to a separatory funnel, add 5 ml of 6% cupferron solution, and extract vanadium in the solution with 25 ml of chloroform. To the aqueous layer add 2 ml of sulfuric acid and 2 ml of nitric acid, and decompose excess cupferron by heating. Cool the solution to room temperature, and 1 to 2 drops of N/10 potassium permanganate and heat for 1 min.
After cooling to room temperature decompose excess permanganate with 0.5 ml of 10% manganese sulfate solution. Then add to the solution 20 ml of deionized water and 2 ml of 0.5% diphenylcarbazide solution, allow to stand for 3 min, and dilute to 25 ml with deionized water. Measure the extinction of the solution at 540 mμ against reagent blank.
The standard deviation was 0.67.View full abstractDownload PDF (977K) -
Takatoshi KONO1970 Volume 19 Issue 8 Pages 1032-1036
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSVarious conditions in the determination of lead by atomic absorption spectroscopy were examined. Lead was extracted as iodide from phosphoric acid solution with MIBK with the extraction rate over 99%. The working conditions for MIBK extracts were: the wavelength 2833 Å, the current of hollow cathods lamp for Pb 9 mA, the slit width 0.18 mm, air pressure 1.8 kg/cm2 (12l/min) and acetylene pressure 0.5 kg/cm2 (2l/min). In the aqueous solution, the optimum air pressure was 1.8 kg/cm2 (13l/min) and acetylene pressure 0.5 kg/cm2 (3.5l/min).
By the extraction method, the sensitivity was increased five-fold compared to that by the aqueous medium. The method was applied to the determination of lead in cast iron, free cutting aluminum alloy and zinc die cast with satisfactory results.View full abstractDownload PDF (730K) -
Fujio MAEDA, Toyoo HAYASAKA1970 Volume 19 Issue 8 Pages 1036-1040
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA method for the determination of microgram quantities of tungsten in iron, molybdenum and titanium by X-ray fluorescence analysis was given, in which tungsten was separated from the matrix metals by phenylfluorone with germanium as the coprecipitant after molybdenum and titanium had been masked respectively with EDTA and hydrogen peroxide.
The precipitation was done most successfully in 1% sulfuric acid or hydrochloric acid, and the precipitate was collected on a membrane filter.
The recommended method was more rapid and sensitive than other chemical and spectrographic methods.View full abstractDownload PDF (852K) -
Masaro SHIMIZU, Keiichiro HOZUMI1970 Volume 19 Issue 8 Pages 1041-1049
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA statistical study on analytical error of an automatic carbon, hydrogen, and nitrogen analyzer, CHN Corder MT-2, which involves a detector system of differential thermal conductometry, has been carried out under normal operations of the analyzer, the component sources of analytical error being evaluated quantitatively in the form of variance. By considering the possible sources of error including A) sample weight, B) bar-gram reading, C) atmospheric pressure, D) temperature of detector oven, E) base signal, F) bridge supply voltage and G) other functions, it was proved that the contributions of F) + G) to the over-all analytical error were several times higher than the sum of contributions of A)E).
It was apparent that the relative stability of the output voltage from the variable D. C. power supplier became higher with increasing voltage. By elevating the bridge supply voltage from 2.1 V to 6.7 V with accompanying change of bridge current from 73 mA to 200 mA and by attenuating, at the same time, the resulting high output signal from the bridge circuit suitably at the input terminal of the given recorder, the precision of analytical results was remarkably improved. The contributions of F) + G) were thus reduced to 1/4 of the initial value. A further investigation indicated that the selective contribution of the improved precision of bridge supply voltage to the improvement of analytical precision was comparable to that of the higher S/N ratio resulted from an increase of bridge current.
A regression analysis relating to the bridge currentand the linearity of calibration line revealed that the latter was maintained regardless to the bridge current tested unless the amount of carbon did not exceed 3000 μg. The scattering of plots was somewhat reduced with increased bridge current. Any bias in analytical values was not detected in the analysis of the data obtained from the calibration values determined by using a number of different organic compounds.View full abstractDownload PDF (1413K) -
Determination of chemical components at the ppb level in both polar snow strata. IMasayo MUROZUMI, Clair C. PATTERSON1970 Volume 19 Issue 8 Pages 1049-1056
Published: August 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA minute amount of chlorine (n×10n×102 μg/kg) in melted snow can be determined by a neutron activation method, whose accuracy is within 10% error covering above concentration range with sensitivity 0.006 μg.
This method can distinguish antarctic snow from the other, measure the distribution of the element in the interior snow strata and also detect yearly and seasonal variations of snow character.View full abstractDownload PDF (1415K) -
Determination of chemical components at the ppb level in both polar snow strata. IIMasayo MUROZUMI, Seiji NAKAMURA, Clair C. PATTERSON1970 Volume 19 Issue 8 Pages 1057-1063
Published: August 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSNeutron activation of nuclides can be applied to the measurement of sodium components at the ppb level in liquid samples by irradiating 23Na with thermal neutron to form 24Na, 1.37 and 2.75 MeV γ rays from which are counted. The detection limit of the element by this method is 0.5 ppb and the accuracy is ± 5% in relative error. Sodium concentration in both polar snow strata has been found to be between 5 and 40 ppb affected by yearly and seasonal atmospheric conditions.
Sodium ions at such concentration level also can be quantitatively determined by atomic absorption method after application of successive freezing concentration to the samples, sodium ions being enriched in liquid phase but not in ice phase. The overall detection limit by this method is 0.5 ppb and the accuracy is-10% in relative error, sodium components in fine particles such as volcanic ashes and clays being occluded, unlike sodium ions, in ice phase.View full abstractDownload PDF (1264K) -
Sigeru NAKAMURA1970 Volume 19 Issue 8 Pages 1064-1068
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSPolystyrene gels for gel permeation chromatography (GPC) were prepared and their separation efficiencies were discussed.
Gels are classified into three types-non solvent modified gels, good solvent modified gels and poor solvent modified gels.
The non solvent modified gels were effective in the separation of materials of relatively low molecular weight-organics or low molecular weight polymers (M. W. below several hundreds).
On the solvent modified gels, the porosities of gels were correlated with the solubility parameters of the diluent added upon polymerization.
Good solvent modified gels were suitable for the separation of polymers of molecular weight ranging from several hundreds to several thousands.
With poor solvent (especially isoamyl alcohol-toluene) modified gels, high molecular weight polymers ranging from several thousands to more than 106 M. W. could be separated.View full abstractDownload PDF (824K) -
Sublimatographic separation in gradient temperature tube furnace. IVKoichi EMI, Yasumasa SHIGETOMI, Nobumasa NAKASHIMA, Hideichi TORIGOE1970 Volume 19 Issue 8 Pages 1069-1073
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSublimation in a gradient-temperature tube furnace offers a new possibility for separating analogous compounds which the normal vacuum sublimation method failed to separate. The behavior of chlorophenols when sublimed in it has been investigated, and it was observed that they were sublimed over a fairly narrow range of temperature such as 137124°C for pentachlorophenol, 7049°C for tetrachlorophenol and 5449°C for trichlorophenol.
Pentachlorophenol was separated successfully from tetrachlorophenol, trichlorophenol and-other analogous compounds such as benzoic acid and salicylic acid.
Tetrachlorophenol and trichlorophenol could be separated from many other aromatic compounds but the mutual separation of tetra-and trichlorophenol was impossible because of contamination of sublimed zone.
It was recognized that this method was more convenient than the normal vacuum sublimation for the purification of reagents and the concentration of impurities.View full abstractDownload PDF (881K) -
Analytical studies on pesticides and related compounds. IIAtsushi MURANO1970 Volume 19 Issue 8 Pages 1074-1077
Published: August 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA colorimetric method has been developed for the determination of 3-methylphenyl N-methylcarbamate (MTMC). The MTMC was separated from impurities by thin layer chromatography (TLC), eluted with ethanol and hydrolyzed with potassium hydroxide. After color development with 4-aminoantipyrine and potassium ferricyanide at pH 8.3, MTMC was spectrophotometrically determined by its absorbance at 495 mμ. Results of the analysis of several samples of technical MTMC were about 1% lower than those obtained by thin layer chromatographic separation and spectrophotometric method already reported. On the other hand, the gas chromatographic determination of 4-methylphenyl N-methylcarbamate(PTMC) which was not separated from MTMC by TLC and of which color was not developed with 4-aminoantipyrine indicated that its content in MTMC was about 1% just in accordance with the difference between the value by two methods. The MTMC was thus determined without the interference from PTMC by the proposed method.View full abstractDownload PDF (613K) -
Analytical studies on pesticides and related compounds. IIIAtsushi MURANO1970 Volume 19 Issue 8 Pages 1077-1080
Published: August 05, 1970
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA quantitative analytical method has been developed for the determination of 3, 4-dimethylphenyl N-methylcarbamate (MPMC) and 3-methylphenyl N-methylcarbamate (MTMC) in mixed formulations. Both MPMC and MTMC were extracted with chloroform, separated from impurities by thin layer chromatography, eluted with ethanol and hydrolyzed with potassium hydroxide solution. Total carbamate content was determined by measuring the absorbance at 296.5 mμ, which was an isobestic point of MPMC and MTMC. On the other hand, MTMC was determined colonmetrically after the reactibn with 4-aminoantipyrine at pH 8.3, and MPMC was determined from the difference between total carbamate content and MTMC content. The analysis of a dust formulation indicated that the proposed method gave precise and reproducible results.View full abstractDownload PDF (587K) -
Hiroshi HASHITANI, Hideyo YOSHIDA1970 Volume 19 Issue 8 Pages 1081-1085
Published: August 05, 1970
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSThe spectrophotometric method for determining ammonia nitrogen with thymol which had been reported by the authors has been successfully applied to the determination of as little as 3 ppm of nitrogen in uranium metal and dioxide. The method is also useful for determining nitrogen in uranium nitride, carboni tride and carbide. The absorbance per μg nitrogen was 0.00818 (molar absorptivity=1.15×104) at 670 mμ by the following procedure.
Metal, oxide and carbide containing up to 0.8 g of uranium are dissolved with 20 ml of hydrochloric acid (6 M) and 5 ml of hydrogen peroxide solution (30%). The other samples are dissolved with 10 ml of hydro chloric acid and 5 ml of fluoboric acid (4%), and uranium is then oxidized with a few drops of hydrogen peroxide solution. After decomposition of excess hydrogen peroxide, the solution is evaporated to dryness on a water bath to remove excess acid, and the residue is dissolved with 40 ml of sodium citrate solution (25 w/v%). The pH of the solution is adjusted to 9.810.3 with sodium hydroxide solution (2 M) and 2 ml of sodium hydrogen carbonate (0.06 M)-sodium carbonate (0.075 M) buffer solution. Then, 0.5 ml of sodium hypochlorite solution containing 0.3% active chlorine is added with stirring. After 20 seconds, 2.5 ml of a freshly prepared mixture of the equal volumes of thymol solution (10% in acetone) and sodium hydroxide solution (1 M) is added. After addition of 4 ml of acetone, the resultant solution is transferred to a 100 ml measuring flask and diluted to the mark with water. After standing 1.5 hours in darkness, the absorbance of the colored solution is measured against the blank at 670 mμ.View full abstractDownload PDF (914K) -
Quantitative spot analysis. IAkira FUJITA, Tsutomu HASUIKE, Shigeyuki OTA1970 Volume 19 Issue 8 Pages 1086-1091
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThree types of solute stains were obtained by spotting a solution gradually on a filter paper, i. e., (I) a round spot of solute separated from its solvent, (II) a ring stain of solute and (III) a round spot of unseparated solute and solvent. The following equations were derived for the type (I),
log[M]σ=kDv*+log kD-log(1+kDv*) +log[M]φ where [M]σ: concentration of solution (mmol/l), [M]φ: amount of solution absorbed per unit area of filter paper (mmol/cm2), v*: retention of solution per unit area of filter paper (ml/cm2) after diffusion of the solution, and kD: s*/V*, in which V* is amount of solution added (ml) and s* is area of the spot after diffusion, and hence log[M]σ_??_log kD+log[M]φ, when kD is small, and log[M]σ_??_kDv*+log[M]φ/v*, when kD is large.
The determination was possible by using above two equations. For example, the equation was applied satisfactorily to the determination of saccharin. The presence of dulcin gaining the spot of type (III) did not interfere with the determination, and saccharin and sodium cyclamate also of type (I) could be determined simultaneously with only a little modification of the procedure.View full abstractDownload PDF (980K) -
Kenji MOTOJIMA, Tadashi YAMAMOTO, Hiroshi MUTO, Yoshiharu KATO1970 Volume 19 Issue 8 Pages 1091-1093
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA spectrophotometric method is described for determination of both aluminum and iron in the presence of plutonium. Plutonium is removed from nitric acid solution by extraction with tributyl phosphate. After masking any residual plutonium with hydrogen peroxide, oxinates of aluminum and iron are extracted with chloroform at pH 4.65.2. The extract is washed with potassium cyanide solution to remove copper and nickel. Then, by measuring the absorbances of the organic phase at 390 and 470 mμ, aluminum and iron are determined. By this method, 4 μg of aluminum and 4 μg of iron in the presence of 1 g of plutonium can be determined.View full abstractDownload PDF (528K) -
Tadaoki OKUMOTO, Tsugio TAKEUCHI, Shin TSUGE1970 Volume 19 Issue 8 Pages 1093-1095
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn analytical method for determining composition of styrene-butadiene copolymers was studied by pyrolysis-gas chromatography.
Relative yield of styrene in copolymer was calculated from the corresponding peaks appearing on the pyrogram at 520°C by making correction for relative sensitivity of the flame ionization detector.
The relationship between the yield (wt%) of styrene and the composition (wt%) of copolymers was linear. The composition of the copolymers was determined by using this relation within 0.6 wt% of mean absolute deviation.View full abstractDownload PDF (476K) -
Masakichi NISHIMURA, Katsuhiko MATSUNAGA, Katsumi MATSUDA1970 Volume 19 Issue 8 Pages 1096-1097
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSOne of the most widely used colorimetric methods for the determination of nitrite is the one involving formation of a red azo-dye.
It has been found by the authors that the azo-dye, having positive charge, is quantitatively extracted into carbon tetrachloride by coupling with the negatively charged ion of alkylbenzenesulfonate. Thus, the sensitivity becomes several times higher in this method than in the ordinary method.
To a 50 ml sample solution are added 1 ml of 1% sulfanilamide in 1.2M hydrochloric acid solution and 1 ml of 0.1% N-1-naphthylethylenediamine dihydrochloride aqueous solution. After 10 min, 5 ml of carbon tetrachloride and 1 ml of 0.03% dodecylbenzenesulfonate aqueous solution are added. The azo-dye is extracted by shaking for 3 min, and the absorbance is measured at 525 mμ.
This method is applied to the determination of trace amount of nitrite in fresh water.View full abstractDownload PDF (290K) -
[in Japanese]1970 Volume 19 Issue 8 Pages 1098-1109
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese], [in Japanese], [in Japanese]1970 Volume 19 Issue 8 Pages 1110-1119
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese], [in Japanese], [in Japanese]1970 Volume 19 Issue 8 Pages 1119-1127
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese], [in Japanese]1970 Volume 19 Issue 8 Pages 1128-1132
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese], [in Japanese]1970 Volume 19 Issue 8 Pages 1132-1141
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
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[in Japanese]1970 Volume 19 Issue 8 Pages 1142-1152
Published: August 05, 1970
Released on J-STAGE: May 29, 2009
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